CN106423276B - A kind of preparation method of nitrogen-doped carbon nickel-loaded Fenton catalyst - Google Patents
A kind of preparation method of nitrogen-doped carbon nickel-loaded Fenton catalyst Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/18—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
- B01J31/1805—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing nitrogen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0203—Impregnation the impregnation liquid containing organic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/086—Decomposition of an organometallic compound, a metal complex or a metal salt of a carboxylic acid
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
- C02F2001/46138—Electrodes comprising a substrate and a coating
- C02F2001/46142—Catalytic coating
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
Abstract
The invention discloses a kind of preparation methods of nitrogen-doped carbon nickel-loaded Fenton catalyst; it is that will be put into Muffle furnace after carbon materials pre-treatment; it is heat-treated 1h at 350 DEG C; it is immersed after cooling in the aqueous solution of nickel salt and aminocarboxylic acid compounds; solution is evaporated completely at 50 DEG C after ultrasonic disperse 0.5h, then 12h is dried in vacuo at 40 DEG C, the material after drying is put into tube furnace; under nitrogen protection through high-temperature heat treatment, Ni/N-C composite materials are obtained.Ni/N-C Fentons catalyst prepared by the present invention is as a concentration of 25mgL of Fenton cathode material catalytic degradation‑1Rhodamine B solution, degradation rate is up to 100% in 5h.
Description
One, technical field
It is in carbon material surface original the present invention relates to a kind of preparation method of nitrogen-doped carbon nickel-loaded Fenton catalyst
Position modification obtains nitrogen-doped carbon load nickel composite material, and is applied to organic wastewater as Fenton catalyst
Degradation treatment.
Two, background technology
The principle of Fenton catalytic oxidation technologies is that the oxygen that will be dissolved in the water is generated in the cathodic reduction of electrolytic cell
H2O2, and decomposed under the action of the catalyst such as iron and generate hydroperoxyl radical and hydroxyl radical free radical oxidation organic pollution, the technology
Key is the high catalytic activity of cathode material.The material that can be used for Fenton cathode has graphite, carbon-PTFE oxygen diffusion electricity
Pole and three-diemsnional electrode such as carbon graphite felt, activated carbon fiber, glassy carbon, sponge carbon and carbon nanotube etc..
Carbon graphite felt is due to being easy to get with larger three-dimensional active surface, structural integrity, industry and being easy to catalyst
Load with regeneration the advantages that and be widely used in handle waste water in toxic or persistent organic pollutants, as dyestuff, phenols,
Insecticide, drug and refuse leachate etc..It is the catalytic activity for further increasing Fenton electrode surface, scientific research work at present
Author has carried out a large amount of research in terms of improving the electro-chemical activities such as electrode surface oxygen content or specific surface area, such as heat treatment,
Acid processing (Shen et al., Electrochim.Acta.2014,132,37-41；Miao et al.,
Chem.Eng.J.2014,250,312-318), chemistry and electrochemical oxidation (Zhou et al.,
Electrochim.Acta.2014,140,376-383), organically-modified (Wang et al., Carbohydrate
Polymers,2011,86,1807-1813；Zhang et al.,Electrochim.Acta.,2008,53,5155-5161)
Metal or metal oxide supported (Wang et al., Appl.Catal.B:Environ.,2009,89,111-117；Li et
Al., J.Hazard.Mater., 2009,164,18-25), patent CN 103928689A are reported in normal temperature air cathodic fuel
Galvanic anode spontaneous oxidation ferrous ion, and be prepared for there are different Fenton catalytic activity by heat treatment FeOOH/C,
Fe2O3/C、Fe3O4/ C carbon-supported nano ferric oxide composite materials.
Three, invention content
The present invention is intended to provide a kind of preparation method of nitrogen-doped carbon nickel-loaded Fenton catalyst, first using dipping
The complex adsorption that method forms nickel ion and aminocarboxylic acids ligand is multiple to carbon materials surface, then by being thermally treated resulting in Ni/N-C
Condensation material.Using the composite material as a concentration of 25mgL of Fenton cathode material catalytic degradation-1Rhodamine B solution, 5h
Inside make its degradation rate up to 100%, and keeps preferable stability.
The preparation method of nitrogen-doped carbon nickel-loaded Fenton catalyst of the present invention, includes the following steps：
It will be put into Muffle furnace after carbon materials pre-treatment, 1h be heat-treated at 350 DEG C, immerses nickel salt and aminocarboxylic acids after cooling
In the aqueous solution of compound, solution is evaporated completely at 50 DEG C after ultrasonic disperse 0.5h, is then dried in vacuo at 40 DEG C
Material after drying is put into tube furnace by 12h, under nitrogen protection through high-temperature heat treatment, obtains Ni/N-C composite materials.It will
Ni/N-C Fentons catalyst prepared by the present invention is as a concentration of 25mgL of Fenton cathode material catalytic degradation-1's
Rhodamine B solution, degradation rate is up to 100% in 5h.
The carbon materials are selected from carbon fiber, carbon felt or carbon cloth.
The method of the carbon materials pre-treatment is first to use 1molL-1Salt acid soak 0.5h, then with acetone soak 0.5h.
The molar ratio of nickel salt and aminocarboxylic acid compounds is in the aqueous solution of the nickel salt and aminocarboxylic acid compounds
1：1~6；The nickel salt is selected from nickel nitrate, nickel acetate, nickel chloride or nickel sulfate；The aminocarboxylic acid compounds are ethylenediamine
One kind in tetraacethyl and its sodium salt (EDTA), nitrilotriacetic acid (NTA) or diethylene-triamine pentaacetic acid (DTPA) etc.；Nickel salt and
The amount of nickel salt accounts for the 10~80% of carbon materials quality in terms of the quality of nickel simple substance in the aqueous solution of aminocarboxylic acid compounds.
The flow velocity of nitrogen is 30~100mLs in high-temperature heat treatment process-1。
The high-temperature heat treatment is to be heat-treated 0.5~3h in 500~900 DEG C.
Fenton catalysis degeneration experiment of the present invention is carried out in a dual chamber electrolytic cell, passes through matter between the anode chamber and the cathode chamber
Proton exchange separates, and Ni/N-C composite materials are cathode, and carbon-point is anode, 0.05molL-1Na2SO4For electrolyte.It will
25mg·L-1Rhodamine B solution be added to cathode chamber after, with 30mls-1Flow velocity blast air from bottom, conducting wire is used in combination
The anode and cathode of battery is connected and accesses 2V DC sources, every 1h sampling analysis degradation effect of organic compound.Degradation rate reaches in 5h
100%.
Compared with the prior art, beneficial effects of the present invention are embodied in：
1, preparation method of the present invention is simple, easy to operate, and the period is short.
2, the present invention is coordinated using aminocarboxylic acid compounds and nickel salt, reducing atmosphere is not necessarily to, by being once heat-treated
It is nitrogen co-doped that nickel can be formed, play the role of concerted catalysis.
3, Ni/N-C composite material large specific surface areas prepared by the present invention, when being catalyzed reaction applied to Fenton, energy
Enough quick adsorption organic pollutions simultaneously implement fast degradation near electrode, can be applied to the drop of higher concentration organic pollution
Solution, and the recyclability of catalyst is good.
Four, it illustrates
Fig. 1 is the different amplification SEM photograph of Ni/N-C composite materials prepared by embodiment 1；
Fig. 2 is the X-ray diffractogram of Ni/N-C composite materials prepared by embodiment 1；
Fig. 3 is that Ni/N-C composite materials prepared by embodiment 1 are urged as continuous recycle 6 times of Fenton cathode material
Change the concentration curve figure of rhodamine B degradation, the wherein initial concentration of rhodamine B is 25mgL-1, each degradation time
For 5h.
Five, specific implementation mode
Embodiments of the present invention are described in detail below in conjunction with portion of techniques scheme：
Embodiment 1：
It is 3 × 3cm to take area2Carbon felt 0.6g, use 1molL respectively-1Hydrochloric acid and acetone soak 0.5h, then by it
It is put into Muffle furnace and is heat-treated 1h at 350 DEG C, immersed after cooling and contain 0.16molL-1Nickel nitrate and 0.48molL-1EDTA
50mL aqueous solutions in, moisture is slowly steamed into method to when having crystal precipitation at 50 DEG C after ultrasonic disperse 0.5h, takes out material simultaneously
It is dried in vacuo 12h at 40 DEG C；Material after drying is put into tube furnace, is 80mLs in flow velocity-1Nitrogen atmosphere under, 500
DEG C heat treatment 3h, obtain Ni/N-C composite materials.
In the dual chamber electrolytic cell that a volume is 250mL, separated by proton exchange membrane between the anode chamber and the cathode chamber, it is above-mentioned
The Ni/N-C composite materials of preparation be cathode, a diameter of 6mm, long 4cm carbon-point be anode, 0.05molL-1Na2SO4For electricity
Xie Zhi.25mgL is added in the cathode chamber of electrolytic cell-1Rhodamine B solution and with 30mls-1Flow velocity blast sky from bottom
The anode and cathode of battery is connected with conducting wire and accesses 2V DC sources by gas, and the degradation rate for powering on rhodamine B in rear 5h reaches
100%.
Embodiment 2：
It is 3 × 3cm to take area2Carbon felt 0.6g, use 1molL respectively-1Hydrochloric acid and acetone soak 0.5h, then by it
It is put into Muffle furnace and is heat-treated 1h at 350 DEG C, immersed after cooling and contain 0.02molL-1Nickel acetate and 0.12molL-1NTA
50mL aqueous solutions in, moisture is slowly steamed into method to when having crystal precipitation at 50 DEG C after ultrasonic disperse 0.5h, takes out material simultaneously
It is dried in vacuo 12h at 40 DEG C；Material after drying is put into tube furnace, is 30mLs in flow velocity-1Nitrogen atmosphere under, 700
DEG C heat treatment 2h after obtain Ni/N-C composite materials.
In the dual chamber electrolytic cell that a volume is 250mL, separated by proton exchange membrane between the anode chamber and the cathode chamber, it is above-mentioned
The Ni/N-C composite materials of preparation be cathode, a diameter of 6mm, long 4cm carbon-point be anode, 0.05molL-1Na2SO4For electricity
Xie Zhi.25mgL is added in the cathode chamber of electrolytic cell-1Rhodamine B solution and with 30mls-1Flow velocity blast sky from bottom
The anode and cathode of battery is connected with conducting wire and accesses 2V DC sources by gas, and the degradation rate for powering on rhodamine B in rear 4h reaches
100%.
Embodiment 3：
It is 3 × 3cm to take area2Carbon felt 0.6g, use 1molL respectively-1Hydrochloric acid and acetone soak 0.5h, then by it
It is put into Muffle furnace and is heat-treated 1h at 350 DEG C, immersed after cooling and contain 0.05molL-1Nickel chloride and 0.05molL-1DTPA
50mL aqueous solutions in, moisture is slowly steamed into method to when having crystal precipitation at 50 DEG C after ultrasonic disperse 0.5h, takes out material simultaneously
It is dried in vacuo 12h at 40 DEG C；Material after drying is put into tube furnace, is 100mLs in flow velocity-1Nitrogen atmosphere under,
Ni/N-C composite materials are obtained after 900 DEG C of heat treatment 0.5h.
In the dual chamber electrolytic cell that a volume is 250mL, separated by proton exchange membrane between the anode chamber and the cathode chamber, it is above-mentioned
The Ni/N-C composite materials of preparation be cathode, a diameter of 6mm, long 4cm carbon-point be anode, 0.05molL-1Na2SO4For electricity
Xie Zhi.25mgL is added in the cathode chamber of electrolytic cell-1Rhodamine B solution and with 30mls-1Flow velocity blast sky from bottom
The anode and cathode of battery is connected with conducting wire and accesses 2V DC sources by gas, and the degradation rate for powering on rhodamine B in rear 4h reaches
100%.
Claims (6)
1. a kind of preparation method of nitrogen-doped carbon nickel-loaded Fenton catalyst, it is characterised in that include the following steps：
It will be put into Muffle furnace after carbon materials pre-treatment, 1h be heat-treated at 350 DEG C, immerses nickel salt and aminocarboxylic acids chemical combination after cooling
In the aqueous solution of object, solution is evaporated completely at 50 DEG C after ultrasonic disperse 0.5h, 12h is then dried in vacuo at 40 DEG C, it will
Material after drying is put into tube furnace, under nitrogen protection through high-temperature heat treatment, obtains Ni/N-C composite materials；
The nickel salt is selected from nickel nitrate, nickel acetate, nickel chloride or nickel sulfate；The aminocarboxylic acid compounds are ethylenediamine tetrem
One kind in acid and its sodium salt, nitrilotriacetic acid or diethylene-triamine pentaacetic acid.
2. preparation method according to claim 1, it is characterised in that：
The carbon materials are selected from carbon fiber, carbon felt or carbon cloth.
3. preparation method according to claim 1, it is characterised in that：
The method of the carbon materials pre-treatment is first to use 1molL-1Salt acid soak 0.5h, then with acetone soak 0.5h.
4. preparation method according to claim 1, it is characterised in that：
The molar ratio of nickel salt and aminocarboxylic acid compounds is 1 in the aqueous solution of the nickel salt and aminocarboxylic acid compounds：1~
6；In the aqueous solution of nickel salt and aminocarboxylic acid compounds the amount of nickel salt accounted in terms of the quality of nickel simple substance carbon materials quality 10~
80%.
5. preparation method according to claim 1, it is characterised in that：
The flow velocity of nitrogen is 30~100mLs in high-temperature heat treatment process-1。
6. preparation method according to claim 1, it is characterised in that：
The high-temperature heat treatment is to be heat-treated 0.5~3h in 500~900 DEG C.
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| CN106925219A (en) * | 2017-04-20 | 2017-07-07 | 兰州交通大学 | A kind of preparation method of magnetic carbon composite adsorbing material |
| CN109305880B (en) * | 2017-07-28 | 2021-09-07 | 中国石油化工股份有限公司 | Synthetic method of alcohol compound |
| CN110255697B (en) * | 2019-06-26 | 2021-11-19 | 合肥工业大学 | Preparation of nitrogen-doped carbon anode and application of nitrogen-doped carbon anode in catalytic wet air oxidation |
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